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Analysis method for determining rebamipide related substances by using HPLC

An analytical method and mobile phase technology used in the field of analytical chemistry to achieve good peak shape

Active Publication Date: 2020-08-28
苏州正济药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although the quality control of rebamipide-related substances is currently included in the Pharmacopoeia, it is impossible to take into account the impurities produced during the synthesis of the following four processes in one analytical method:

Method used

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  • Analysis method for determining rebamipide related substances by using HPLC
  • Analysis method for determining rebamipide related substances by using HPLC
  • Analysis method for determining rebamipide related substances by using HPLC

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Embodiment 1: contrast HPLC analytical method

[0059] High performance liquid chromatography: Shimadzu;

[0060] Chromatographic column: Shiseido CAPCELL PAK UG120 250*4.6mm*5μm;

[0061] Mobile phase: Dissolve 2.44g of sodium 1-decanesulfonate in 1000ml of water, then add 1000ml of methanol and 10ml of phosphoric acid;

[0062] Detection wavelength: 232nm;

[0063] Flow rate: adjust the flow rate so that the retention time of rebamipide is about 12 minutes;

[0064] Column temperature: 25°C;

[0065] Injection volume: 10μl;

[0066] isocratic elution;

[0067] Mixed solution preparation: take appropriate amount of rebamipide, impurity A, impurity B, impurity C, and impurity D, and diluent [water-pH6.0 0.05mol / L phosphate buffer-methanol (7:7:6 )] dissolved and diluted to make a solution containing about 0.4 mg of rebamipide per 1 ml, and 0.04 mg of impurity A, impurity B, impurity C, and impurity D respectively, and shake well.

[0068] Test results: See the at...

Embodiment 2

[0069] Embodiment 2: contrast HPLC analytical method

[0070] High performance liquid chromatography: Shimadzu;

[0071] Chromatographic column: Wakopak Wakosil-II 3C18 4.6mm*150mm;

[0072] Mobile phase A: Phosphate buffer solution of pH 6.2 (weigh 9.08g of potassium dihydrogen phosphate and dissolve in 1000ml of water, weigh 9.46g of anhydrous disodium hydrogen phosphate and dissolve in 1000ml of water. Take 800ml of potassium dihydrogen phosphate solution and add Mix 200ml of disodium hydrogen phosphate solution evenly. If necessary, adjust the pH to 6.2 with potassium dihydrogen phosphate solution or disodium hydrogen phosphate solution) Add 750ml of water to 300ml and mix well;

[0073] Mobile phase B: acetonitrile;

[0074] Detection wavelength: 222nm;

[0075] Column temperature: 25°C;

[0076] Injection volume: 10μl;

[0077] Gradient elution: the flow rate was adjusted so that the retention time of rebamipide was about 20 minutes, see Table 5.

[0078] table 5 ...

Embodiment 3

[0082] Embodiment 3: contrast HPLC analytical method

[0083] High performance liquid chromatography: Agilent 1260;

[0084] Chromatographic column: Kromasil 100-5C18 4.6mm*250mm, 5μm;

[0085] Mobile phase: methanol: phosphate buffer (6.8g of potassium dihydrogen phosphate, add 152ml of 0.1mol / L sodium hydroxide solution, add 20ml of tetrabutylammonium hydroxide 10% aqueous solution, dilute to 1000ml with water, adjust pH to 6.5 with phosphoric acid) = 52:48;

[0086] Detection wavelength: 235nm;

[0087] Flow rate: 0.8ml / min;

[0088] Column temperature: 40°C;

[0089] Injection volume: 20μl;

[0090] isocratic elution;

[0091] Mixed solution preparation: take appropriate amount of rebamipide, impurity A, impurity B, impurity C, and impurity D, dissolve and dilute with mobile phase to make about 0.2 mg of rebamipide, impurity A, and impurity B per 1 ml , Impurity C, and Impurity D are 0.02mg solutions, shake well.

[0092] Test results: See the attached image 3 , ...

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Abstract

The invention relates to the technical field of analytical chemistry, and discloses an analysis method for determining rebamipide related substances by using HPLC. According to the analysis method, octadecylsilane chemically bonded silica is used as a reversed phase chromatographic column of a filler, a buffer salt solution is used as a mobile phase A, the buffer salt solution, methanol and tetrahydrofuran are used as a mobile phase B, gradient elution is carried out on a rebamipide sample solution, and HPLC analysis is carried out. The analysis method provided by the invention can effectivelyseparate rebamipide and related substances thereof, so that impurity peaks and rebamipide peaks are not overlapped, the peak shape is good, the separation requirement is met, and the method is suitable for controlling related substances and researching impurities.

Description

technical field [0001] The invention relates to the technical field of analytical chemistry, in particular to an analytical method for determining related substances of rebamipide by HPLC. Background technique [0002] Rebamipide (±) 2-(4-chlorobenzamido)-3-[2(1H)-quinolinone-4]propionic acid is a prostaglandin derivative and a new type of gastric mucosal protective agent , its CAS number is: 90098-04-7, and its molecular formula is C 19 h 15 ClN 2 o 4 , molecular weight: 370.79, chemical structure: [0003] [0004] Rebamipide is an anti-ulcer drug developed by Otsuka Pharmaceutical Company of Japan. The trade name was first launched in Japan as an oral protective anti-ulcer drug. Prevent and treat peptic ulcer by strengthening the defense function of gastric mucosa; increase gastric mucosal prostaglandin content, increase gastric membrane blood flow, and increase gastric mucus; inhibit gastric back diffusion and promote gastric alkali secretion; eliminate and inh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34G01N30/86
CPCG01N30/02G01N30/34G01N30/8634G01N30/8637
Inventor 侯叶婷董梦飞
Owner 苏州正济药业有限公司
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